تفاعل #66573

ord-3a98d504e8e4451b97bff5363160ad09

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwas added
  2. 2
    درجة الحرارةThe resulting slurry was cooled to approximately 0° C.
  3. 3
    ترشيحthen filtered
  4. 4
    أخرىThe filtrate was evaporated in vacuo
  5. 5
    أخرىthe residue was purified by chromatography (silica, 1-4% MeOH/DCM as eluent)

الإجراء التجريبي

(S)+-2-methylpiperazine (10 g) was dissolved in acetonitrile (140 ml) and cooled to 5-10° C. whereupon triethylamine (35 ml) was added, followed by drop wise addition of a solution of trityl chloride 27.9 (g) in DCM (80 ml). The reaction was stirred for 1 h at room temperature. The resulting slurry was cooled to approximately 0° C. then filtered. The filtrate was evaporated in vacuo and the residue was purified by chromatography (silica, 1-4% MeOH/DCM as eluent) to give the sub-title compound (29 g).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08524715B2uspto-grants-2013_09